#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:44:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179304 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/01/4320171.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4320171
loop_
_publ_author_name
'Yucang Liang'
'Maochun Hong'
'Weiping Su'
'Rong Cao'
'Wenjian Zhang'
_publ_section_title
;
 Preparations, Structures, and Magnetic Properties of a Series of Novel
 Copper(II)-Lanthanide(III) Coordination Polymers via Hydrothermal
 Reaction
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4574
_journal_page_last               4582
_journal_paper_doi               10.1021/ic0100929
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C42 H58 Cu3 Gd2 N6 O44'
_chemical_formula_weight         1856.06
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.333(2)
_cell_angle_beta                 101.675(2)
_cell_angle_gamma                105.61
_cell_formula_units_Z            1
_cell_length_a                   10.1194(6)
_cell_length_b                   10.5763(5)
_cell_length_c                   14.3500(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      1.47
_cell_volume                     1430.77(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_sigmaI/netI    0.1876
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7634
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    3.509
_exptl_crystal_colour            blue-purle
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             919
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.856
_refine_diff_density_min         -2.091
_refine_diff_density_rms         0.256
_refine_ls_extinction_coef       0.0033(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         5028
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1545
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0963P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2317
_reflns_number_gt                2699
_reflns_number_total             5028
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100929_6.cif
_cod_data_source_block           l
_cod_original_cell_volume        1430.80(13)
_cod_database_code               4320171
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd Gd 0.49906(10) 0.24897(9) 0.49565(6) 0.0346(4) Uani 1 1 d . . .
Cu1 Cu 0.0000 0.0000 0.0000 0.0468(9) Uani 1 2 d S . .
Cu2 Cu 0.3023(2) 0.20960(19) -0.03302(14) 0.0329(6) Uani 1 1 d . . .
O1 O 0.7073(16) 0.3691(15) 0.4450(11) 0.084(5) Uani 1 1 d . . .
H1A H 0.6836 0.4091 0.4013 0.126 Uiso 1 1 calc R . .
O2 O 0.2966(14) 0.3071(13) 0.5328(9) 0.061(4) Uani 1 1 d . . .
H2A H 0.3214 0.3568 0.5845 0.092 Uiso 1 1 calc R . .
O3 O 0.7146(15) 0.2299(15) 0.5979(12) 0.090(5) Uani 1 1 d . . .
H3A H 0.6945 0.1849 0.6394 0.135 Uiso 1 1 calc R . .
O4 O 0.2790(14) 0.0839(12) 0.4035(9) 0.062(4) Uani 1 1 d . . .
H4A H 0.2946 0.0434 0.3574 0.093 Uiso 1 1 calc R . .
O11 O -0.028(4) 0.306(3) 0.4124(17) 0.186(14) Uani 1 1 d . . .
O12 O 0.013(2) 0.117(2) 0.3877(13) 0.114(7) Uani 1 1 d . . .
O13 O 0.0267(13) 0.1486(10) -0.0746(9) 0.045(3) Uani 1 1 d . . .
O14 O -0.0048(15) 0.3459(13) -0.0769(10) 0.064(4) Uani 1 1 d . . .
O21 O 0.4520(13) -0.0831(13) -0.4057(8) 0.048(3) Uani 1 1 d . . .
O22 O 0.4369(14) 0.1228(11) -0.3856(8) 0.047(3) Uani 1 1 d . . .
O23 O 0.2862(12) 0.0718(9) 0.0471(7) 0.034(3) Uani 1 1 d . . .
O24 O 0.3216(11) -0.1252(10) 0.0562(8) 0.032(3) Uani 1 1 d . . .
O31 O 0.4190(17) 0.5549(13) 0.3977(9) 0.066(4) Uani 1 1 d . . .
O32 O 0.4175(16) 0.3467(12) 0.3642(9) 0.059(4) Uani 1 1 d . . .
O33 O 0.3112(13) 0.3455(12) -0.1125(8) 0.043(3) Uani 1 1 d . . .
O34 O 0.3252(13) 0.5590(11) -0.1072(8) 0.043(3) Uani 1 1 d . . .
O01 O -0.007(4) 0.277(6) -0.280(3) 0.37(3) Uani 1 1 d . . .
O02 O 0.056(5) 0.147(4) 0.587(3) 0.32(2) Uani 1 1 d . . .
O03 O 0.970(3) 0.403(6) 0.574(3) 0.37(4) Uani 1 1 d . . .
O04 O 0.2599(18) 0.4797(18) -0.3043(12) 0.095(6) Uani 1 1 d . . .
O05 O 0.2516(17) -0.0906(16) 0.2368(10) 0.085(5) Uani 1 1 d . . .
O06 O 0.0000 0.5000 0.0000 0.048(5) Uani 1 2 d S . .
N1 N 0.0029(14) 0.1413(14) 0.1041(11) 0.038(4) Uani 1 1 d . . .
N2 N 0.3352(14) 0.0794(12) -0.1263(9) 0.032(3) Uani 1 1 d . . .
N3 N 0.3308(14) 0.3522(13) 0.0736(9) 0.033(3) Uani 1 1 d . . .
C11 C -0.001(4) 0.230(4) 0.368(3) 0.119(13) Uani 1 1 d . . .
C12 C -0.002(2) 0.231(2) 0.2558(17) 0.066(6) Uani 1 1 d . . .
C13 C -0.008(2) 0.354(2) 0.2217(18) 0.074(8) Uani 1 1 d . . .
H13A H -0.0134 0.4245 0.2629 0.089 Uiso 1 1 calc R . .
C14 C -0.0052(19) 0.3654(18) 0.1196(16) 0.058(6) Uani 1 1 d . . .
H14A H -0.0053 0.4429 0.0939 0.070 Uiso 1 1 calc R . .
C15 C -0.0028(17) 0.2532(16) 0.0678(12) 0.031(4) Uani 1 1 d . . .
C16 C 0.004(2) 0.135(2) 0.1974(16) 0.068(6) Uani 1 1 d . . .
H16A H 0.0082 0.0571 0.2205 0.082 Uiso 1 1 calc R . .
C17 C 0.004(2) 0.2513(17) -0.0360(16) 0.053(5) Uani 1 1 d . . .
C21 C 0.4258(19) 0.0143(19) -0.3596(12) 0.040(4) Uani 1 1 d . . .
C22 C 0.3944(17) -0.0101(16) -0.2670(11) 0.032(4) Uani 1 1 d . . .
C23 C 0.3925(17) -0.1236(16) -0.2269(12) 0.037(4) Uani 1 1 d . . .
H23A H 0.4122 -0.1930 -0.2608 0.044 Uiso 1 1 calc R . .
C24 C 0.3625(17) -0.1381(14) -0.1384(11) 0.032(4) Uani 1 1 d . . .
H24A H 0.3581 -0.2171 -0.1139 0.038 Uiso 1 1 calc R . .
C25 C 0.3392(16) -0.0338(16) -0.0874(11) 0.029(4) Uani 1 1 d . . .
C26 C 0.3603(16) 0.0915(14) -0.2119(11) 0.030(4) Uani 1 1 d . . .
H26A H 0.3558 0.1684 -0.2374 0.036 Uiso 1 1 calc R . .
C27 C 0.3117(19) -0.0340(17) 0.0124(12) 0.036(4) Uani 1 1 d . . .
C31 C 0.406(2) 0.4541(18) 0.3397(12) 0.042(4) Uani 1 1 d . . .
C32 C 0.3737(17) 0.4624(14) 0.2334(11) 0.033(4) Uani 1 1 d . . .
C33 C 0.364(2) 0.5782(14) 0.1988(11) 0.041(5) Uani 1 1 d . . .
H33A H 0.3733 0.6544 0.2406 0.049 Uiso 1 1 calc R . .
C34 C 0.341(2) 0.5778(17) 0.1040(14) 0.063(6) Uani 1 1 d . . .
H34A H 0.3322 0.6548 0.0805 0.076 Uiso 1 1 calc R . .
C35 C 0.3306(17) 0.4683(15) 0.0386(12) 0.032(4) Uani 1 1 d . . .
C36 C 0.3501(16) 0.3483(15) 0.1652(10) 0.029(4) Uani 1 1 d . . .
H36A H 0.3484 0.2678 0.1868 0.035 Uiso 1 1 calc R . .
C37 C 0.3168(18) 0.4613(16) -0.0685(12) 0.031(4) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O21 Gd O31 148.7(5) 2_655 2_666 ?
O21 Gd O22 95.4(4) 2_655 1_556 ?
O31 Gd O22 92.8(4) 2_666 1_556 ?
O21 Gd O32 95.6(4) 2_655 . ?
O31 Gd O32 94.3(4) 2_666 . ?
O22 Gd O32 145.9(5) 1_556 . ?
O21 Gd O2 139.5(5) 2_655 . ?
O31 Gd O2 71.8(5) 2_666 . ?
O22 Gd O2 74.8(4) 1_556 . ?
O32 Gd O2 75.9(5) . . ?
O21 Gd O1 77.3(5) 2_655 . ?
O31 Gd O1 77.2(5) 2_666 . ?
O22 Gd O1 140.5(5) 1_556 . ?
O32 Gd O1 73.5(5) . . ?
O2 Gd O1 134.1(5) . . ?
O21 Gd O3 77.3(5) 2_655 . ?
O31 Gd O3 76.8(6) 2_666 . ?
O22 Gd O3 71.7(5) 1_556 . ?
O32 Gd O3 142.3(5) . . ?
O2 Gd O3 132.2(5) . . ?
O1 Gd O3 68.8(5) . . ?
O21 Gd O4 69.6(4) 2_655 . ?
O31 Gd O4 141.7(5) 2_666 . ?
O22 Gd O4 79.0(5) 1_556 . ?
O32 Gd O4 74.8(5) . . ?
O2 Gd O4 70.0(4) . . ?
O1 Gd O4 131.0(5) . . ?
O3 Gd O4 132.9(5) . . ?
O13 Cu1 O13 180.0(6) 2 . ?
O13 Cu1 N1 97.2(5) 2 . ?
O13 Cu1 N1 82.8(5) . . ?
O13 Cu1 N1 82.8(5) 2 2 ?
O13 Cu1 N1 97.2(5) . 2 ?
N1 Cu1 N1 180.0(8) . 2 ?
O33 Cu2 O23 177.9(5) . . ?
O33 Cu2 N3 85.5(5) . . ?
O23 Cu2 N3 94.2(5) . . ?
O33 Cu2 N2 95.8(5) . . ?
O23 Cu2 N2 85.0(5) . . ?
N3 Cu2 N2 162.9(6) . . ?
C17 O13 Cu1 114.0(12) . . ?
C21 O21 Gd 176.4(12) . 2_655 ?
C21 O22 Gd 144.0(10) . 1_554 ?
C27 O23 Cu2 114.7(10) . . ?
C31 O31 Gd 166.1(14) . 2_666 ?
C31 O32 Gd 143.4(12) . . ?
C37 O33 Cu2 114.6(10) . . ?
C16 N1 C15 120.0(16) . . ?
C16 N1 Cu1 129.7(14) . . ?
C15 N1 Cu1 110.2(11) . . ?
C26 N2 C25 120.3(13) . . ?
C26 N2 Cu2 129.4(11) . . ?
C25 N2 Cu2 110.2(10) . . ?
C36 N3 C35 120.8(14) . . ?
C36 N3 Cu2 129.3(11) . . ?
C35 N3 Cu2 109.9(10) . . ?
O11 C11 O12 128(4) . . ?
O11 C11 C12 124(3) . . ?
O12 C11 C12 107(3) . . ?
C16 C12 C13 119(2) . . ?
C16 C12 C11 126(3) . . ?
C13 C12 C11 115(2) . . ?
C12 C13 C14 118.9(17) . . ?
C15 C14 C13 113.8(19) . . ?
N1 C15 C14 124.4(18) . . ?
N1 C15 C17 115.7(14) . . ?
C14 C15 C17 119.8(17) . . ?
C12 C16 N1 124(2) . . ?
O14 C17 O13 124(2) . . ?
O14 C17 C15 121.0(17) . . ?
O13 C17 C15 115.1(16) . . ?
O22 C21 O21 124.2(15) . . ?
O22 C21 C22 121.3(15) . . ?
O21 C21 C22 114.2(15) . . ?
C23 C22 C26 115.9(14) . . ?
C23 C22 C21 126.0(15) . . ?
C26 C22 C21 118.1(15) . . ?
C22 C23 C24 122.2(15) . . ?
C25 C24 C23 118.6(14) . . ?
C24 C25 N2 120.9(14) . . ?
C24 C25 C27 124.0(14) . . ?
N2 C25 C27 115.0(13) . . ?
N2 C26 C22 121.9(14) . . ?
O24 C27 O23 124.4(15) . . ?
O24 C27 C25 120.7(14) . . ?
O23 C27 C25 114.8(14) . . ?
O31 C31 O32 124.0(16) . . ?
O31 C31 C32 118.2(15) . . ?
O32 C31 C32 117.8(15) . . ?
C33 C32 C36 117.6(14) . . ?
C33 C32 C31 122.5(14) . . ?
C36 C32 C31 119.9(14) . . ?
C34 C33 C32 118.3(15) . . ?
C33 C34 C35 123.3(16) . . ?
N3 C35 C34 117.4(15) . . ?
N3 C35 C37 115.3(13) . . ?
C34 C35 C37 127.3(15) . . ?
N3 C36 C32 122.2(14) . . ?
O34 C37 O33 123.6(15) . . ?
O34 C37 C35 121.7(15) . . ?
O33 C37 C35 114.2(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd O21 2.301(10) 2_655 ?
Gd O31 2.303(13) 2_666 ?
Gd O22 2.342(11) 1_556 ?
Gd O32 2.345(12) . ?
Gd O2 2.433(11) . ?
Gd O1 2.436(14) . ?
Gd O3 2.439(14) . ?
Gd O4 2.458(12) . ?
Cu1 O13 1.972(11) 2 ?
Cu1 O13 1.972(11) . ?
Cu1 N1 2.002(14) . ?
Cu1 N1 2.002(14) 2 ?
Cu2 O33 1.911(11) . ?
Cu2 O23 1.932(10) . ?
Cu2 N3 1.965(13) . ?
Cu2 N2 1.970(12) . ?
O11 C11 1.10(3) . ?
O12 C11 1.29(3) . ?
O13 C17 1.27(2) . ?
O14 C17 1.22(2) . ?
O21 C21 1.288(19) . ?
O21 Gd 2.301(10) 2_655 ?
O22 C21 1.223(19) . ?
O22 Gd 2.342(11) 1_554 ?
O23 C27 1.292(18) . ?
O24 C27 1.215(18) . ?
O31 C31 1.25(2) . ?
O31 Gd 2.303(13) 2_666 ?
O32 C31 1.249(19) . ?
O33 C37 1.306(19) . ?
O34 C37 1.209(18) . ?
N1 C16 1.34(2) . ?
N1 C15 1.35(2) . ?
N2 C26 1.315(18) . ?
N2 C25 1.374(19) . ?
N3 C36 1.295(18) . ?
N3 C35 1.370(19) . ?
C11 C12 1.61(4) . ?
C12 C16 1.27(3) . ?
C12 C13 1.44(3) . ?
C13 C14 1.49(3) . ?
C14 C15 1.35(2) . ?
C15 C17 1.50(3) . ?
C21 C22 1.46(2) . ?
C22 C23 1.38(2) . ?
C22 C26 1.43(2) . ?
C23 C24 1.38(2) . ?
C24 C25 1.37(2) . ?
C25 C27 1.51(2) . ?
C31 C32 1.51(2) . ?
C32 C33 1.38(2) . ?
C32 C36 1.42(2) . ?
C33 C34 1.33(2) . ?
C34 C35 1.39(2) . ?
C35 C37 1.51(2) . ?
